CN105566102A - Process for directly producing gallic acid through acid hydrolysis of gallnuts - Google Patents
Process for directly producing gallic acid through acid hydrolysis of gallnuts Download PDFInfo
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- CN105566102A CN105566102A CN201410551737.2A CN201410551737A CN105566102A CN 105566102 A CN105566102 A CN 105566102A CN 201410551737 A CN201410551737 A CN 201410551737A CN 105566102 A CN105566102 A CN 105566102A
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- acid
- gallnuts
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- acid hydrolysis
- hydrolysis
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Abstract
The invention provides a production process for extracting gallic acid from gallnuts. The gallnuts are used as a starting raw material, acid hydrolysis is directly performed by using sulfuric acid, and residue removal is performed by adopting a special preprocessing mode and a reaction material proportion and selecting a refine waste carbon processing and filter-pressing mode. The complicated process of firstly extracting tannic acid of gallnuts in a traditional process is omitted, production procedures are greatly simplified, the product yield and content are improved, and the production cost is reduced obviously.
Description
Technical field
The present invention relates to field of fine chemical, a kind of technique extracting gallic acid from Turkey-galls is particularly provided.
Background technology
Gallic acid is commonly called as amasses wealth by heavy taxation acid, and chemical name is Gallic Acid (3,4,5 one frihydroxybenzoicacid), and it, as the intermediate of Chemicals and pharmaceutical prod, is widely used in the fields such as medicine, chemical industry, printing and dyeing, food.Turkey-galls is the main raw material producing gallic acid.Traditional production technique is that starting raw material carries out normal pressure acid hydrolysis and produces with Chinese gallotanninic acid.This method needs first by the screening of Turkey-galls raw material crushing, lixiviate, evaporation, obtained Chinese gallotanninic acid, again sour water alkali is carried out to the Weibull concentrated solution of gained, crystallisation by cooling obtains crude product, gallic acid finished product (chemistry of forest product and industry is obtained after refining, 2000,20 (2): 71-82).This method and technology circuit process is complicated, and the production cycle is long, and facility investment is large, and yield is low, and raw material and labor force consume high.At the beginning of the nineties, also there are preparation technology (chemistry of forest product and industry, 1995,15 (1): 1-8 of drawing powder to be raw materials for production with tower; Chinese patent CN1083532,1994), played vital role when Turkey-galls price is high at that time.But fall after rise with Turkey-galls price in recent years, most producer abandons this technique.The comparatively advanced method now adopted is the preparation technology (ZL93114806 of the direct basic hydrolysis of Bian, 5), it is higher that this technique has product yield, main raw material Turkey-galls consumes low feature, but due to its auxiliary material caustic soda and salt acid consumption also high, when current caustic soda and hydrochloric acid price higher, its feature fails formation advantage.
Summary of the invention
For overcoming above-mentioned shortcoming, object of the present invention is just that providing a kind of directly carries out with Turkey-galls the technique that gallic acid is produced in acid hydrolysis, and not only technique is comparatively simple for it, and yield is high, and raw material consumption amount is low.
For achieving the above object, containing acid hydrolysis in present invention process, it is characterized in that: processing step comprises:
First Turkey-galls is pulverized, with 70 ° of C water soakings 2 hours, then direct enriching 30
4carry out acid hydrolysis.
Useless carbon decoloring 30 minutes, press filtration, crystallisation by cooling, deviates from waste hydrolyzed liquid;
With activated carbon decolorizing, temperature is 85 ° of C, 0.5 hour time, and adopt EDTA complex reaction 0.5 hour, then through vacuum filtration, crystallisation by cooling, vacuum-drying forms.
Reacting material concentration has material impact to hydrolysis degree and filtration velocity, and through repetition test, optimum hydrolysis reaction material concentration of the present invention is Turkey-galls: water: dense Stickers 0
4=1
:4
:0.3 time and temperature are the essential condition of hydrolysis reaction.Temperature is high, the time is long, is conducive to carrying out completely of hydrolysis reaction.But under long-time and high-temperature condition, hydrolysate gallic acid generation side reaction, has a direct impact product yield and quality.Through test, the present invention determines that hydrolysis optimum temps and time conditions are: 128.C、3h。
Present invention omits in classical acid hydrolysis process and first will extract Weibull from Turkey-galls and carry out the working procedures such as concentrating, directly adopt acid-hydrolyzed one-step technology, enormously simplify life ' produce process, ratio defective product significantly improves, and reaches 41.6%.And initial cost can be saved in a large number, reduce production cost, there are good economic advantages.Meanwhile, owing to have employed special impurity removal and purification method, output content also significantly improves, and reaches more than 99.0%.
Embodiment
The concrete steps of this technique are:
2200 premium on currency are injected steeping tank, and dropped in water by 550 kilograms of Turkey-galls of making powdery, stir evenly, heat up 70 ° of C, soaks 2 hours;
Soak solution is imported souring tank, enriching H
2s0
4160 kilograms, stir evenly, be warmed up to 128 ° of C, be hydrolyzed 3 hours;
After hydrolysis terminates, add refining useless carbon decoloring 30 minutes, by pulling the press filtration of frame pressure filter, filtrate crystallisation by cooling, deviating from waste hydrolyzed liquid and obtaining gallic acid crude product;
Will not eat sour fine work and add pure water 2200 liters, with gac refinery decolorization 1 hour under 85 ° of C, add EDTA complex reaction 0.5 hour, vacuum filtration, filtrate crystallisation by cooling, sloughs refinement mother liquor, obtains gallic acid and to wet crystal.The refinement mother liquor sloughed is recyclable makes hydrating solution;
It is dry that the crystal that will wet drops into Vacuumdrier, obtains gallic acid fine work 229.2 kilograms.
Claims (3)
1. a technique for producing gallic acid by direct acid hydrolysis of gallnut, containing acid hydrolysis in technique, it is characterized in that, processing step comprises.
First pulverized by gall nut, with 70 ° of C water soakings 2 hours, then direct enriching went out 30
4carry out acid hydrolysis;
With useless carbon decoloring 30 minutes, press filtration, crystallisation by cooling, deviates from waste hydrolyzed liquid;
With activated carbon decolorizing, temperature is 85 ° of C, 0.5 hour time, and adopt EDTA complex reaction 0.5 hour, then through vacuum filtration, crystallisation by cooling, vacuum-drying forms.
2. technique for producing gallic acid by direct acid hydrolysis of gallnut according to claim 1, is characterized in that, acid-hydrolyzed material ratio is gallnut extract: water: dense H
2s0
4=1
:4:0.3.
3. technique for producing gallic acid by direct acid hydrolysis of gallnut according to claim 1, is characterized in that, acid-hydrolyzed optimal temperature is 128 ° of C, 3 hours time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410551737.2A CN105566102A (en) | 2014-10-17 | 2014-10-17 | Process for directly producing gallic acid through acid hydrolysis of gallnuts |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410551737.2A CN105566102A (en) | 2014-10-17 | 2014-10-17 | Process for directly producing gallic acid through acid hydrolysis of gallnuts |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105566102A true CN105566102A (en) | 2016-05-11 |
Family
ID=55876813
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410551737.2A Pending CN105566102A (en) | 2014-10-17 | 2014-10-17 | Process for directly producing gallic acid through acid hydrolysis of gallnuts |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105566102A (en) |
-
2014
- 2014-10-17 CN CN201410551737.2A patent/CN105566102A/en active Pending
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160511 |
|
| WD01 | Invention patent application deemed withdrawn after publication |